CN103282555A - Method of manufacturing silicon single crystal, silicon single crystal, and wafer - Google Patents
Method of manufacturing silicon single crystal, silicon single crystal, and wafer Download PDFInfo
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- CN103282555A CN103282555A CN2011800633441A CN201180063344A CN103282555A CN 103282555 A CN103282555 A CN 103282555A CN 2011800633441 A CN2011800633441 A CN 2011800633441A CN 201180063344 A CN201180063344 A CN 201180063344A CN 103282555 A CN103282555 A CN 103282555A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 34
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- 229910052796 boron Inorganic materials 0.000 claims abstract description 69
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- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 49
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/04—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their crystalline structure, e.g. polycrystalline, cubic or particular orientation of crystalline planes
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/14—Heating of the melt or the crystallised materials
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02524—Group 14 semiconducting materials
- H01L21/02532—Silicon, silicon germanium, germanium
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Abstract
To provide a method of manufacturing silicon single crystal by manufacturing with a Czochralski method, p-type silicon single crystal from which a wafer having high resistivity, good radial uniformity of resistivity and less variation in resistivity can be obtained. P-type silicon single crystal 2 is grown with a Czochralski method from an initial silicon melt in which boron concentration is not higher than 4E14 atoms/cm3 and a ratio of phosphorus concentration to boron concentration is not lower than 0.42 and not higher than 0.50.
Description
Technical field
The present invention relates to silicon single-crystal manufacture method, silicon single-crystal and wafer, particularly relate to method, silicon single-crystal and wafer by Czochralski manufactured silicon single-crystal.
Background technology
The power apparatus that is installed on automobile, the household electrical appliance etc. should have high resistance to pressure, and the resistance of substrate influences its characteristic.Therefore, require silicon wafer as substrate to have high resistivity and its variation is little.
If by Czochralski method growing p-type silicon single-crystal, wherein add boron as impurity, then because boron for the segregation coefficient of silicon single-crystal less than 1, so concentrate in silicon melt at boron during the single crystal growing.So the boron concentration in the silicon single-crystal increases along with the growth of monocrystalline.Therefore, in top and the end of the central shaft during crystal growth of gained silicon single-crystal (ingot) (below be called " central shaft during the crystal growth "), the resistivity of silicon single-crystal changes.
, a kind ofly be added into the initial stage silicon melt and be suppressed at the technology of the change in resistance on the crystal growth direction by Czochralski method growing crystal by the phosphorus that will be equivalent to 25 to 30% boron concentration thereby exist because the conventional art of the change in resistance that segregation causes as be used for suppressing.No. 3931956 special permission of Japan's special permission communique relates to this conventional art.
The problem to be solved in the present invention
Yet above-mentioned conventional art can't be realized the radially change in resistance between homogeneity and the wafer of stricter resistivity, and that this is the silicon single-crystal wafer of power apparatus purposes is desired.
Address this problem by the present invention.
Summary of the invention
Solve the means of described problem
The problems referred to above of the present invention solve by the following method.
The silicon single-crystal manufacture method is characterized in that, is not more than 4E14 atom/cm by the Czochralski method by boron concentration wherein
3And the ratio of phosphorus concentration and boron concentration is not less than 0.42 and be not more than 0.50 initial stage silicon melt growing p-type silicon single-crystal.
Technique effect of the present invention
Can pass through Czochralski manufactured P type silicon single-crystal, can obtain to have high resistivity thus, the good resistivity wafer of homogeneity and little change in resistance radially.
Description of drawings
Figure 1 shows that for the synoptic diagram of enforcement according to the silicon single-crystal manufacturing equipment of the silicon single-crystal manufacture method of one embodiment of the invention.
Figure 2 shows that for the schema of implementing according to the silicon single-crystal manufacture method of this embodiment of the present invention.
Fig. 3 is the measuring result that concerns between the curing degree of the analog result that concerns between the interior impurity concentration of the curing degree that shows silicon single-crystal and silicon single-crystal and silicon single-crystal and the resistivity and the figure of analog result.
Fig. 4 is the figure of relation between the curing degree that shows silicon single-crystal and the resistivity with the analog result of the dependency of initial stage silicon melt P/B ratio.
Figure 5 shows that in the silicon solid-liquid interface when the Czochralski method growing silicon single crystal and at the position on the central shaft during the crystal growth and the graph of a relation between the resistivity.
Embodiment
At length set forth silicon single-crystal manufacture method, silicon single-crystal and wafer according to one embodiment of the invention with reference to the accompanying drawings.
Relate to manufacturing for the wafer of power apparatus according to the silicon single-crystal manufacture method of the present embodiment.
Mainly for following reason, the wafer that is used to form power apparatus should meet following standard, and resistivity is not less than 50 Ω cm, and the change in resistance between the wafer is not more than 10%, and the resistivity radial variations in the wafer is not more than 3%.
At first, because power apparatus is applied high-voltage, so power apparatus should have high resistance to pressure.In addition, the resistance to pressure of power apparatus is relevant with the numerical value of the resistivity of the wafer that is used to form power apparatus.Therefore, the wafer for power apparatus should have high resistivity.At present the resistance to pressure of the power apparatus of main flow is not less than 250V, and requires wafer to have to be not less than the resistivity of 50 Ω cm.On the other hand, along with the resistivity change of wafer is big, it is big that the width of depletion layer becomes.The width of depletion layer exceedingly will cause depletion layer to contact with pn knot part in addition greater than device architecture, and causes voltage endurance to reduce.Therefore, in order to improve the resistance to pressure of power apparatus, the resistivity of wafer should be higher, and its variation simultaneously should be little.
Secondly, in power apparatus, provide wherein the transistor that extracts collector current from the back side of silicon substrate (for example IGBT(igbt, Insulated Gate Bipolar Transistor)), the change in resistance of wafer is bigger to the influence of transistor characteristic.Therefore, thus being used to form this type of transistorized wafer should be that resistivity is high and change the little wafer of characteristics of transistor in regulating scope that make.
Again, because the device producer can't screen wafer when receiving wafer, the resistivity radial variations in the wafer causes the screening productive rate after forming device low.Therefore, in order to suppress to increase cost owing to device yield reduces, the wafer that is used for device should have little change in resistance.
Figure 1 shows that for the synoptic diagram of enforcement according to the silicon single-crystal manufacturing equipment of the silicon single-crystal manufacture method of the present embodiment.
As shown in Figure 1, silicon single-crystal manufacturing equipment 100 is the equipment of making silicon single-crystal by Czochralski method (below be called " CZ method ").The drive unit 10 that silicon single-crystal manufacturing equipment 100 has the crucible 30 that holds silicon melt and makes silicon single-crystal 2 liftings, makes silicon single-crystal 2 rotations and crucible 30 is rotated.Silicon single-crystal manufacturing equipment 100 has the control device 1 that the rotation of the rotation of the lifting that makes silicon single-crystal 2 by drive unit 10, silicon single-crystal 2 and crucible 30 is controlled.
Silicon single-crystal manufacturing equipment 100 has the chamber 20 that holds crucible 30 and silicon single-crystal 2, along the well heater 42 of the sidewall setting of crucible 30, be arranged on the well heater 44 of crucible 30 belows and 20 sidewall and bottom arrange along the chamber lagging material 26.
Silicon single-crystal manufacturing equipment 100 has from the chamber line 3 that 20 top hangs down and the chuck 6 that online 3 top is used for keeping crystal seed 8 is set.
Silicon single-crystal manufacturing equipment 100 has the flow regulation pipe 60 of discharging the gas discharge outlet 24 of chamber 20 and being used for regulating the flow of rare gas element for the rare gas element that rare gas element is imported gas introduction port 22 in the chamber 20, is used for importing.Rare gas element for example is Ar gas.
Provide silicon melt 32 by polysilicon as raw material.
In the present embodiment, in order to make p-type silicon single-crystal 2, boron (B) is added into as p-type impurity (acceptor) be called " initial stage silicon melt " below the silicon melt 32(at single crystal growing initial stage).In addition, further add phosphorus (P), its be n type impurity (donor) and for the segregation coefficient of silicon single-crystal 2 less than boron.Therefore, will be to increase and prevent that the direction of the central shaft of resistivity during crystal growth from changing (increase of change in resistance rate) for the resistivity that makes silicon single-crystal 2 as the impurity opposite with the conduction type of boron and for the reason that the segregation coefficient of silicon single-crystal 2 is added into the initial stage silicon melt less than the phosphorus of boron.
In addition, in the present embodiment, further suppress the variation of resistivity on the direction of the central shaft during the crystal growth, thereby further be suppressed at perpendicular to the resistivity radial variations (increase of change in resistance rate) in the plane of the central shaft during crystal growth of silicon single-crystal 2.For this reason, make the initial stage silicon melt satisfy boron concentration and be not more than 4E14 atom/cm
3And the ratio of phosphorus concentration and boron concentration is not less than 0.42 and be not more than 0.50, below to this detailed description.
Crucible 30 is for example formed by synthetic quartz glass.Crucible 30 is connected with the axle 34 of support crucible in its bottom.Flow regulation pipe 60 is arranged on crucible 30 tops, and is the shape of frustum basically.
Figure 2 shows that for the schema of implementing according to the silicon single-crystal manufacture method of the present embodiment.
Be method by CZ manufactured silicon single-crystal 2 according to the silicon single-crystal manufacture method of the present embodiment, it is included in the rare gas element filling step S1 that produces inert gas atmospheres in the chamber 20, the melt that generates silicon melt 32 generates step S2, the silicon monocrystal growth step S3 of growing silicon single crystal 2 and the separating step S4 that silicon single-crystal 2 is separated with silicon melt 32.
In rare gas element filling step S1, with chamber 20 sealings, import rare gas element and in chamber 20, produce inert gas atmosphere via gas introduction port 22, by the vacuum pump (not shown) gas is discharged from described chamber via gas discharge outlet 24 simultaneously.Should be noted that in each following step by rare gas element being supplied in the chamber 20 and chamber 20 is remained in the inert gas atmosphere.
After rare gas element filling step S1, generate among the step S2 at melt, make the raw material fusing that is supplied in the crucible 30 by well heater 42 and 44, thereby produce initial stage silicon melt 32.
In the present embodiment, boron and phosphorus are added into silicon melt 32, be not more than 4E14 atom/cm thereby make initial stage silicon melt 32 satisfy boron concentration
3And the ratio of phosphorus concentration and boron concentration is not less than 0.42 and be not more than 0.50.
Because initial stage silicon melt 32 has described composition, so the resistivity of silicon single-crystal 2 is increased, and the change in resistance rate of the central axis L 1 during the crystal growth is further reduced, and can make perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth and reduce.In other words, can growing p-type silicon single-crystal 2, wherein the resistivity of the central axis L 1 during the crystal growth is not less than 50 Ω cm, the change in resistance rate of the central axis L 1 during the crystal growth is not more than 10%, and is not more than 3% perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth.
At this, by following formula (1) definition change in resistance rate.
Change in resistance rate=(the Zui Da Zhi – resistivity minimum value of resistivity)/resistivity maximum value
Formula (1)
After generating step S2, melt in silicon monocrystal growth step S3, also immerses wherein by the surface that wrapping machine 12 makes crystal seed 8 be moved downward to silicon melt 32.Then, make silicon single-crystal 2 from silicon melt 32 growth, the straight barrel sections 4 of the ingot of growing silicon single crystal 2 thus by wrapping machine 12.Silicon single-crystal 2 and crucible 30 rotate with opposite directions.
In the present embodiment, the growth velocity of silicon single-crystal 2 is not less than 0.9mm/min in silicon monocrystal growth step S3, and the rate of cooling of crystal edge part can be at least 1.4 times of rate of cooling of germ nucleus part.At this, rate of cooling refer to by will be on the direction of crystal growth axle from the average temperature gradient of fusing point to 1350 ℃ (℃/mm) multiply by the numerical value that crystal growth rate (mm/min) calculates, this average temperature gradient be during the crystal growth at the mean value in the scope of fusing point to 1350 ℃.Crystal growth rate is not preferred less than 0.9mm/min, and this is because productive rate is poor.The rate of cooling of crystal edge part is less than 1.4 times of cooling efficiency variation that can cause silicon single-crystal of the rate of cooling of germ nucleus part, so crystal growth rate becomes less than 0.9mm/min, and the productive rate variation.Because the ability of attainable silicon single-crystal growth equipment, the upper limit of crystal growth rate is 1.9mm/min, and the upper limit of the rate of cooling of crystal edge part is 2 times of rate of cooling of germ nucleus part.
The barrel portion that the straight barrel section 4 of ingot is silicon single-crystal 2, its diameter is substantially constant in the direction of the central axis L during crystal growth 1 of silicon single-crystal 2.In case silicon single-crystal 2 after forming conical portion, reach predefined diameter, the straight barrel section 4 of the ingot of then growing.
After growth ingot straight barrel section 4 in separating step S4, the rolling of stop line 3, and by making crucible 30 declines that silicon single-crystal 2 is separated with silicon melt 32.
According to the present embodiment, can make p-type silicon single-crystal 2, wherein the resistivity of the central axis L 1 during the crystal growth is not less than 50 Ω cm, the change in resistance rate of the central axis L 1 during the crystal growth is not more than 10%, is not more than 3% perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth.
The reason that realizes described effect by the present embodiment is described below.
Fig. 3 A is the figure of the analog result that concerns between the curing degree that shows silicon single-crystal and the impurity concentration in the silicon single-crystal.Fig. 3 B is the measuring result that concerns between the curing degree that shows silicon single-crystal and the resistivity and the figure of analog result.Dotted line among Fig. 3 B is represented actual measured results, and solid line is represented analog result.
As shown in Figure 3A, separately boron is being added under the situation of initial stage silicon melt, along with silicon monocrystal growth (being that curing degree becomes greatly), the impurity concentration in the silicon single-crystal increases with exponential manner.Therefore, shown in Fig. 3 B, along with silicon monocrystal growth, the resistivity of silicon single-crystal reduces.
This is because boron is about 0.78 for the segregation coefficient k of silicon single-crystal, and less than 1, therefore along with silicon monocrystal growth, the boron in the silicon melt concentrates, and the ratio of introducing the boron in the silicon single-crystal becomes big.
Separately phosphorus is being added under the situation of initial stage silicon melt, similarly, along with silicon monocrystal growth, the impurity concentration in the silicon single-crystal increases with exponential manner.On the other hand, phosphorus is about 0.38 for the segregation coefficient k of silicon single-crystal, less than the segregation coefficient of boron.Therefore, along with the growth of silicon single-crystal, the ratio (speed) that the phosphorus in the silicon melt concentrates is greater than the situation of boron.Therefore, along with the growth of silicon single-crystal, the ratio of resistivity decreased is also greater than the situation of adding boron.
Because boron is p-type impurity, cause in silicon single-crystal, producing the room as the p-type current carrier so add boron to silicon single-crystal.Because phosphorus is n type impurity, cause in silicon single-crystal, producing electronics as n type current carrier so add phosphorus to silicon single-crystal.
In the silicon single-crystal that has added boron and phosphorus, the reciprocal current carrier of the conduction type of generation is cancelled out each other.Therefore, by in making the semi-conductive process of p-type, phosphorus being added into silicon single-crystal together with boron, can reduce the p-type carrier density in the silicon single-crystal, and resistivity is increased.
In addition, along with the growth of silicon single-crystal, the ratio that impurity concentration increases under the situation of adding phosphorus is greater than the situation of adding boron.Therefore, the increase of the p-type carrier density that the increase by boron concentration causes is offset in the increase of the n type carrier density that causes by the increase by phosphorus concentration along with the growth of silicon single-crystal, thereby can avoid the reduction along with the growth resistivity of silicon single-crystal.In other words, by the ratio of phosphorus concentration in the initial stage silicon melt and boron concentration (below be called " P/B ratio ") is set at suitable numerical value, thereby can avoid the reduction along with the growth resistivity of silicon single-crystal.Because it is enough low to be added into the concentration of the boron of initial stage silicon melt and phosphorus, so think that boron and phosphorus are independently of one another for the silicon single-crystal segregation.
Particularly, as shown in Figure 3A, by selecting the P/B ratio of initial stage silicon melt, make that in the silicon monocrystal growth process difference of boron concentration and phosphorus concentration is constant in the silicon single-crystal, can make the numerical value of resistivity keep constant along with the growth of silicon single-crystal, shown in Fig. 3 B.
Fig. 3 B has shown that in the early stage it is 1.6E14 atom/cm that silicon melt satisfies boron concentration
3And the P/B ratio is measuring result and the analog result of resistivity under 0.45 the situation.
Fig. 4 is the figure of the analog result of the dependency of the curing degree that shows silicon single-crystal and the relation between the resistivity and initial stage silicon melt P/B ratio.At this, the ratio of the resistivity among Fig. 4 is by following formula (2) expression.
The resistivity maximum value formula (2) of the ratio of the resistivity=resistivity minimum value of this crystal of – (the Dian Zu of specific curing degree Shuai)/this crystal
According to the analog result shown in Fig. 4 as can be seen, curing degree is being limited at 0 to 0.80 o'clock, be set at 0.42 to 0.55 by the P/B ratio with the initial stage silicon melt, the change in resistance rate of the central shaft during the crystal growth is reduced to below 10%.Yet as described below, reduce in order to make perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth, the P/B ratio should be set at 0.42 to 0.50.Also describe below and curing degree is limited in 0 to 0.80 reason.
At this, the P/B ratio of silicon melt is 0.42 to 0.50 o'clock in the early stage, along with the curing degree that is grown in of silicon single-crystal 2 is about the phenomenon (point that below resistivity is begun to increase is called " point of inflection (flexion point) ") that the resistivity that occurred silicon single-crystal 2 at 0.7 o'clock begins to increase.This phenomenon shows that the p-type current carrier (room) in the silicon single-crystal 2 begins to reduce, and this is because the increment rate of phosphorus is above the increment rate of boron in the silicon single-crystal 2.
In the present embodiment, by until producing the point of inflection, the change in resistance rate of the central shaft during the crystal growth is reduced.After producing the point of inflection, as long as the phosphorus concentration in the silicon single-crystal is no more than boron concentration, then silicon single-crystal also remains the p-type conduction type, can not have problems when silicon single-crystal is used the wafer that acts on power apparatus.
Further reduce by the change in resistance rate that makes the central shaft during the crystal growth thus, can make perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth and further reduce.Its reason is described below.
Fig. 5 is the synoptic diagram that is presented at the silicon solid-liquid interface (interface between silicon melt and the silicon single-crystal) when making silicon single-crystal carry out crystal growth by the CZ method.
As shown in Figure 5, the silicon solid-liquid interface when silicon single-crystal 2 carries out crystal growth has the outstanding shape of direction in the central axis L during crystal growth 1 of silicon single-crystal 2.Point A represents the intersection point of present solid-liquid interface and the central axis L during the crystal growth 1.The horizontal section that comprises an A (perpendicular to the cross section of the central shaft during the crystal growth) of some B ' expression silicon single-crystal and the intersection point of the side of silicon single-crystal 2.Point B represents solid-liquid interface in the past and the intersection point of the central axis L during the crystal growth 1.Distance between A and the B is designated as Δ Z, and the difference of the resistivity between A and the B is designated as Δ R.
At this, because each resistivity of solid-liquid interface is constant, so the resistivity that some B and some B ' locate equates.On the other hand, change in resistance amount between the B is corresponding to the change in resistance rate of the central axis L 1 during crystal growth at an A and point, and in an A and the change in resistance amount between the B ' put corresponding to perpendicular to the change in resistance rate in the section A 1 of the central axis L 1 during the crystal growth.Therefore, reduce in order to make perpendicular to the change in resistance rate in the section A 1 of the central axis L 1 during the crystal growth, the obliquity Δ R/ Δ Z of resistivity should reduce on the direction of the central axis L 1 during the crystal growth.Based on the simulation among Fig. 4, reduce effectively for the obliquity that makes resistivity, set the upper limit of curing degree and the P/B ratio is set in the specific scope.Curing degree surpasses 0.80 zone and has resistivity obliquity big when P/B ratio arbitrarily, is therefore surpassing 3% perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth.Curing degree is being limited at 0 to 0.80 o'clock, by the P/B ratio in the initial stage silicon melt is set at more than 0.42 to below 0.50, being below 3% perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth, confirm among the embodiment described as follows.More preferably, curing degree is being limited under 0 to 0.80 the situation, by the P/B ratio being set at more than 0.42 to below 0.47, being below 2% perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth, confirm among the embodiment described as follows.Curing degree is being limited under 0 to 0.80 the situation, by the P/B ratio is set at greater than 0.50 to below 0.55, obliquity in the resistivity of crystal bottom side becomes big, is therefore surpassing 3% perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth.By curing degree is limited in less than 0.80, even the P/B ratio is greater than 0.50 and be not more than 0.55, can be for being not more than 3% perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth.Yet because productive rate is poor, it is not preferred that curing degree is limited in less than 0.80.
Reducing perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth in order to make, thereby the cooling conditions of control silicon single-crystal during crystal growth is realized the solid-liquid interface of even shape that the Δ Z that namely reduces among Fig. 5 also is effective.Yet in the case, the rate of cooling of crystal edge part should be preferably 1 times less than 1.4 times of the rate of cooling of germ nucleus part.As previously mentioned, the reduction of the rate of cooling of edge section causes the cooling efficiency variation of silicon single-crystal.So crystal growth rate becomes less than 0.9mm/min, and the productive rate variation.The present invention can realize little change in resistance during silicon monocrystal growth, and can not reduce productive rate.
Thereby the rate of cooling of the rate of cooling by control crystal edge part and germ nucleus part with the setting value of Δ Z in 5 to 15mm scope, can keep productive rate simultaneously for being not more than 3% perpendicular to the change in resistance rate in the cross section of the central axis L 1 during the crystal growth.Be set in more than 1.4 to below 2.0 by the ratio with the rate of cooling of the rate of cooling of crystal edge part and germ nucleus part, can be with the Numerical Control of Δ Z in 5 to 15mm scope.
According to the present embodiment, can make perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth and reduce, need not to use specific installation, for example in crystal growth, apply the MCZ(magnetic Czochralski in magnetic field, Magnetic field applied CZochralski).Therefore, can suppress manufacturing cost.
In following embodiment, attempt carrying out the actual measurement perpendicular to the change in resistance rate in the section A 1 of the central axis L during crystal growth 1 of silicon single-crystal 2.
Should be noted that the wafer that cuts from the silicon single-crystal that obtains in the present invention can perhaps can use the wafer of having implemented following high-temperature heat treatment directly with the wafer that acts on power apparatus.
High-temperature heat treatment is preferably implemented in non-oxidizing atmosphere, and this is because room or other primary (grown-in) defectives are fully eliminated during can't annealing in oxidizing atmosphere.Non-oxidizing atmosphere refers to not contain the atmosphere such as the oxidizing gas of oxygen, and it comprises inert atmosphere and reducing atmosphere.Inert atmosphere refers to for example be filled with the inert gas atmosphere such as argon, helium, neon, nitrogen etc.Reducing atmosphere refers to wherein exist the atmosphere such as the reducing gas of hydrogen, carbon monoxide, ammonia etc.
To wafer implement heat treated temperature 1150 to 1250 ℃, preferred 1175 to 1215 ℃, more preferably in 1185 to 1200 ℃ the scope.
If silicon substrate is implemented heat treated temperature less than 1150 ℃, then room or other primary defectives can't fully be eliminated during annealing.Alternatively, if this temperature surpasses 1250 ℃, member that then can badly damaged stove.
Wafer is implemented the heat treated time length be not less than 10 minutes and be not more than 2 hours, be preferably and be not less than 30 minutes and be not more than 1.5 hours, more preferably be not less than 50 minutes and be not more than 1 hour.
If wafer was implemented the heat treated time length less than 10 minutes, then room or other primary defectives can't fully be eliminated during annealing.Alternatively, if this time length surpasses 2 hours, productive rate variation then is so be not preferred.
Can use the heat treatment furnace (or reaction chamber) of commercially available acquisition to implement thermal treatment (annealing) in the manufacture method according to the present embodiment, this stove has no particular limits.Should be noted that and to avoid during heating treatment oxide film growth to more than the 2nm that this is because sull adheres to and stoped contraction and the elimination of defective during annealing from the teeth outwards.Particularly, need take following measure, for example minimizing is during heating treatment introduced the amount of the impurity in the atmosphere gas or is reduced as far as possible when inserting silicon wafer in the stove and bring air into from surrounding environment as far as possible.As atmosphere gas to be used, for example be preferably the rare gas that wherein impurity is suppressed at below the 5ppma, for example argon.
The member of the maintenance silicon wafer that uses in the manufacture method according to the present embodiment has no particular limits, and for example uses quartz etc.When annealing temperature excessively reduces, these member apparent damages.So need frequent the replacing, this can cause the increase of manufacturing cost.
Embodiment
Embodiment and comparative example according to the silicon single-crystal manufacture method of this embodiment of the present invention are described below.
Make silicon single-crystal
To be used for growth diameter by the equipment of CZ manufactured silicon single-crystal is the silicon single-crystal (ingot) of 200mm.
At this, the initial stage silicon melt has boron concentration and phosphorus concentration as follows, and crystal seed is immersed in the initial stage silicon melt with growing silicon single crystal.Crystal growth rate is set at 0.9mm/min, and the rate of cooling of crystal edge part is set at 1.9 times of rate of cooling of germ nucleus part.
(1) embodiment 1
Boron and phosphorus are added into the initial stage silicon melt, thereby make boron concentration reach 1.6E14 atom/cm
3, phosphorus concentration reaches 7.2E13 atom/cm
3(ratio of phosphorus concentration and boron concentration is 0.45).
(2) embodiment 2
Boron and phosphorus are added into the initial stage silicon melt, thereby make boron concentration reach 4.0E14 atom/cm
3, phosphorus concentration reaches 1.8E14 atom/cm
3(ratio of phosphorus concentration and boron concentration is 0.45).
(3) embodiment 3
Boron and phosphorus are added into the initial stage silicon melt, thereby make boron concentration reach 1.1E14 atom/cm
3, phosphorus concentration reaches 4.6E13 atom/cm
3(ratio of phosphorus concentration and boron concentration is 0.42).
(4) embodiment 4
Boron and phosphorus are added into the initial stage silicon melt, thereby make boron concentration reach 1.6E14 atom/cm
3, phosphorus concentration reaches 7.5E13 atom/cm
3(ratio of phosphorus concentration and boron concentration is 0.47).
(5) embodiment 5
Boron and phosphorus are added into the initial stage silicon melt, thereby make boron concentration reach 1.6E14 atom/cm
3, phosphorus concentration reaches 8.0E13 atom/cm
3(ratio of phosphorus concentration and boron concentration is 0.50).
(6) comparative example 1
Boron is added into the initial stage silicon melt, thereby makes boron concentration reach 1.0E14 atom/cm
3
(7) comparative example 2
Boron and phosphorus are added into the initial stage silicon melt, thereby make boron concentration reach 1.4E14 atom/cm
3, phosphorus concentration reaches 4.2E13 atom/cm
3(ratio of phosphorus concentration and boron concentration is 0.30).
(8) comparative example 3
Boron and phosphorus are added into the initial stage silicon melt, thereby make boron concentration reach 1.8E14 atom/cm
3, phosphorus concentration reaches 9.9E13 atom/cm
3(ratio of phosphorus concentration and boron concentration is 0.55).
Estimate silicon single-crystal
The central shaft of silicon single-crystal during perpendicular to crystal growth of growth cut into section, form the wafer of cutting thus.Then, extract the wafer of cutting from the position of the direction of a plurality of central shafts during crystal growth, carry out mirror finish then.Make wafer thus.Wafer to gained was implemented pyroprocessing 1 hour in argon gas atmosphere under 1200 ℃.
Center, the radius measured at the wafer of gained by four probe method are that 50mm and radius are the resistivity of the each point of 90mm.
To calculate thus along the change in resistance rate of the central shaft during crystal growth of silicon single-crystal in the measuring result substitution formula (1) of the resistivity of the central spot of each wafer.
In addition, be that 50mm and radius are the measuring result substitution formula (1) of resistivity of the each point of 90mm with center, the radius of each silicon wafer, calculate the resistivity radial variations rate of silicon wafer thus similarly.
The result
(1) embodiment 1
Table 1 has shown the result of embodiment 1.
Table 1 has shown with respect to the curing degree that extracts the position of wafer in the silicon single-crystal of making according to embodiment 1, the resistivity radial variations rate of the resistivity of center wafer and wafer.
Table 1
According to table 1, be not more than 0.80 place at curing degree, minimum value along the resistivity (corresponding to the resistivity of center wafer) of the central shaft of silicon single-crystal during crystal growth is 130 Ω cm, the change in resistance rate of the central shaft during the crystal growth is 7.1%, is 1.4% perpendicular to the maximum value of the change in resistance rate in the cross section of the central shaft during the crystal growth.
In other words, can make silicon single-crystal, wherein the resistivity along the central shaft of silicon single-crystal during crystal growth is not less than 50 Ω cm, the change in resistance rate of the central shaft during the crystal growth is not more than 10%, is not more than 3% perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth.
Should be noted that in the present embodiment the silicon single-crystal that obtains surpasses the resistivity radial variations rate at 0.80 place at curing degree maximum value surpasses 3%.
(2) comparative example 1
Table 2 has shown the result of comparative example 1.
Table 2 has shown with respect to the curing degree that extracts the position of silicon wafer in the silicon single-crystal of making according to comparative example 1, the result of the resistivity radial variations rate of the resistivity of silicon wafer center and silicon wafer.
Table 2
According to table 2, be not more than 0.80 place at curing degree, minimum value along the resistivity (corresponding to the resistivity of center wafer) of the central shaft of silicon single-crystal during crystal growth is not less than 114 Ω cm, the change in resistance rate of the central shaft during the crystal growth is 29.6%, is 4.0% perpendicular to the maximum value of the change in resistance rate in the cross section of the central shaft during the crystal growth.
In other words, can't make silicon single-crystal, wherein the resistivity along the central shaft of silicon single-crystal during crystal growth is not less than 50 Ω cm, the change in resistance rate of the central shaft during the crystal growth is not more than 10%, is not more than 3% perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth.
(3) comparison of embodiment and comparative example
Table 3 has shown the result of embodiment 1 to 5 and comparative example 1 to 3.
Table 3 shown the silicon single-crystal according to each embodiment and each comparative example manufacturing be positioned at the change in resistance rate of the resistivity of center wafer, the central shaft during the crystal growth, perpendicular to the result of the change in resistance rate in the cross section of the central shaft during the crystal growth, together with the concentration that has shown each impurity in the initial stage silicon melt.
Table 3
According to table 3, in embodiment 1 to 5, be not more than 0.80 place at curing degree, along silicon single-crystal in the minimum value of the resistivity of the central shaft during the crystal growth in the scope of 50 to 175 Ω cm, the change in resistance rate of the central shaft during the crystal growth in 4.7 to 8.9% scope, perpendicular to the maximum value of the change in resistance rate in the cross section of the central shaft during the crystal growth in 1.4 to 2.5% scope.
In other words, the silicon single-crystal that obtains in each embodiment can meet the following standard of silicon single-crystal, this standard is required in order to meet for the standard of the silicon single-crystal wafer of power apparatus, the resistivity of the central shaft during the crystal growth is not less than 50 Ω cm, the change in resistance rate of the central shaft during the crystal growth is not more than 10%, is not more than 3% perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth.
In addition, in embodiment 1 to 4, be not more than 0.80 place at curing degree, be not more than 2% perpendicular to the maximum value of the change in resistance rate in the cross section of the central shaft during the crystal growth.
On the other hand, in comparative example 1 to 3, be not more than 0.80 place at curing degree, along silicon single-crystal in the minimum value of the resistivity of the central shaft during the crystal growth in the scope of 114 to 124 Ω cm, the change in resistance rate of the central shaft during the crystal growth in 7.3 to 29.8% scope, perpendicular to the maximum value of the change in resistance rate in the cross section of the central shaft during the crystal growth in 3.3 to 4.0% scope.
In other words, the silicon single-crystal that obtains in comparative example is in the change in resistance rate of the central shaft during crystal growth with perpendicular to the standard that can't meet silicon single-crystal aspect the change in resistance rate in the cross section of the central shaft during the crystal growth, and this standard is required in order to meet for the standard of the silicon single-crystal wafer of power apparatus purposes.
The change in resistance rate of the central shaft during the crystal growth of the silicon single-crystal that attention is made in embodiment 1 to 4 and comparative example 1 to 3 and the relation between the resistivity radial variations rate, basically can confirm the increase along with the change in resistance rate of the central shaft during crystal growth, the tendency that resistivity radial variations rate increases.
According to measuring result confirmation in the above-described embodiments, by the silicon single-crystal manufacture method according to the present embodiment, namely by the boron concentration in the initial stage silicon melt is set in 4E14 atom/cm
3Below the ratio that reaches phosphorus concentration and boron concentration is set in more than 0.42 to below 0.50, can make the p-type silicon single-crystal, wherein be not more than 0.80 place at curing degree, the resistivity of the central shaft during the crystal growth is not less than 50 Ω cm, the change in resistance rate of the central shaft during the crystal growth is not more than 10%, is not more than 3% perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth.
Confirm in addition, by the boron concentration in the initial stage silicon melt is set in 4E14 atom/cm
3Below the ratio that reaches phosphorus concentration and boron concentration is set in more than 0.42 to below 0.47, can make the p-type silicon single-crystal, wherein be not more than 0.80 place at curing degree, the resistivity of the central shaft during the crystal growth is not less than 50 Ω cm, the change in resistance rate of the central shaft during the crystal growth is not more than 10%, is not more than 2% perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth.
Described silicon single-crystal manufacture method, silicon single-crystal and wafer according to this embodiment of the present invention above, the present embodiment obtains following effect.
Can make the p-type silicon single-crystal with the batch productive rate of excellence by the CZ method, wherein the resistivity of the central shaft during the crystal growth is not less than 50 Ω cm, the change in resistance rate of the central shaft during the crystal growth is not more than 10%, is not more than 3% perpendicular to the change in resistance rate in the cross section of the central shaft during the crystal growth.
Claims (10)
1. the silicon single-crystal manufacture method is characterized in that, is not more than 4E14 atom/cm by the Czochralski method by boron concentration wherein
3And the ratio of phosphorus concentration and boron concentration is not less than 0.42 and be not more than 0.50 initial stage silicon melt growing p-type silicon single-crystal.
2. according to the silicon single-crystal manufacture method of claim 1, it is characterized in that, be set in more than 1.4 to below 2.0 by the ratio with the rate of cooling of the centre portions of the rate of cooling of the edge section of silicon single-crystal and silicon single-crystal, thus the growing p-type silicon single-crystal.
3. by the p-type silicon single-crystal of Czochralski method by the initial stage silicon melt growth that is added with boron and phosphorus, it is characterized in that, the resistivity of the central shaft during the crystal growth is not less than 50 Ω cm, and the change in resistance rate of the central shaft during the described crystal growth is not more than 10%.
4. according to the silicon single-crystal of claim 3, it is characterized in that, be not more than 3% perpendicular to the change in resistance rate in the cross section of the central shaft during the described crystal growth.
5. wafer, it is to obtain by cutting into section in the mode perpendicular to the central shaft during the described crystal growth according to the silicon single-crystal of claim 3.
6. wafer, it is to obtain by cutting into section in the mode perpendicular to the central shaft during the described crystal growth according to the silicon single-crystal of claim 4.
7. wafer, it has the sull that is not more than 2nm after thermal treatment, wherein to being not less than 1150 ℃ and be not more than and implement described thermal treatment under 1250 ℃ the temperature and last and be not less than 10 minutes and be not more than 2 hours according to the wafer of claim 5 in non-oxidizing atmosphere.
8. according to the wafer of claim 7, wherein said non-oxidizing atmosphere is that wherein impurity is not more than the rare gas atmosphere of 5ppma.
9. wafer, it has the sull that is not more than 2nm after thermal treatment, wherein to being not less than 1150 ℃ and be not more than and implement described thermal treatment under 1250 ℃ the temperature and last and be not less than 10 minutes and be not more than 2 hours according to the wafer of claim 6 in non-oxidizing atmosphere.
10. according to the wafer of claim 9, wherein said non-oxidizing atmosphere is that wherein impurity is not more than the rare gas atmosphere of 5ppma.
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| PCT/EP2011/069808 WO2012089392A1 (en) | 2010-12-28 | 2011-11-10 | Method of manufacturing silicon single crystal, silicon single crystal, and wafer |
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| CN107419328A (en) * | 2017-08-18 | 2017-12-01 | 晶科能源有限公司 | A kind of preparation method of P-type silicon foundry alloy |
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| WO2017137438A1 (en) * | 2016-02-08 | 2017-08-17 | Topsil Globalwafers A/S | A phosphorus doped silicon single crystal |
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Also Published As
| Publication number | Publication date |
|---|---|
| SG189506A1 (en) | 2013-05-31 |
| US8961685B2 (en) | 2015-02-24 |
| JP2012148949A (en) | 2012-08-09 |
| WO2012089392A1 (en) | 2012-07-05 |
| KR101522480B1 (en) | 2015-05-21 |
| EP2659030B1 (en) | 2015-01-07 |
| EP2659030A1 (en) | 2013-11-06 |
| CN103282555B (en) | 2016-08-17 |
| JP5194146B2 (en) | 2013-05-08 |
| KR20130114696A (en) | 2013-10-17 |
| US20130277809A1 (en) | 2013-10-24 |
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